CN104359845A - Method for measuring content of zinc in rubber by using atomic absorption spectrometer - Google Patents
Method for measuring content of zinc in rubber by using atomic absorption spectrometer Download PDFInfo
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- CN104359845A CN104359845A CN201410671026.9A CN201410671026A CN104359845A CN 104359845 A CN104359845 A CN 104359845A CN 201410671026 A CN201410671026 A CN 201410671026A CN 104359845 A CN104359845 A CN 104359845A
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Abstract
The invention discloses a method for measuring the content of zinc in rubber by using an atomic absorption spectrometer, belonging to the technical field of rubber. The method comprises the following steps: adding a certain amount of nitric acid into a rubber sample for performing microwave digestion; measuring an absorbance value at certain wavelength by using the continuum light source atomic absorption spectrometer, thereby obtaining the concentration of zinc in the sample; and calculating the content of zinc. The method disclosed by the invention is simple, rapid and accurate.
Description
Technical field
The present invention relates to a kind of method of the Zn content measured in rubber, more specifically, relate to after utilizing micro-wave digestion rubber sample, measure the method for the Zn content in rubber with continuum source atomic absorption spectrometer, belong to field of rubber technology.
Background technology
The mensuration of Zn-ef ficiency in environment is mainly contained: EDTA chemistry titration, Atomic absorption, inductively coupled plasma-atomic emissions, X-fluorescence etc., also have a lot for pre-treating method, mainly Wet, dry ashing, environmental pollution is larger, therefore, need a kind of more succinct, fast, accurately, cost is lower, environmental pollution is less, the detection method lower to human injury.Adopt the pre-treating method process rubber sample of micro-wave digestion herein, less to environmental hazard.
Summary of the invention
The object of the invention is to set up a kind of fast, effectively, measure the method for Zn content in rubber accurately.
To achieve these goals, of the present inventionly provide a kind of method measuring Zn content in rubber, the method is applicable to rubber, latex, elastomeric compound and vulcanizate.
Specifically, comprise the steps: according to the method for the Zn content in mensuration rubber of the present invention
(1), drawing standard curve
Prepare 6 ~ 8 different zinc standard series, test with continuum source atomic absorption spectrometer, obtain the typical curve about zinc concentration and absorbance;
(2), sample preparation and measurement
Be placed in counteracting tank by glue sample freeze grinding to be measured, gelatinous substance amount to be measured is designated as m, adds salpeter solution, and composite can is put into micro-wave digestion workstation and carried out micro-wave digestion after having assembled; After having cleared up, counteracting tank is taken out and exit in ventilation, until do not have yellow smog to emerge; Move in volumetric flask with deionized water gradation by digestion solution, constant volume shakes up, and volume is designated as V, measures absorbance at continuum source atomic absorption spectrometer;
(3), calculate
On the typical curve of step (1) gained, corresponding zinc concentration C is searched according to the sample solution absorbance of step (2) gained
t;
The content of zinc in rubber is calculated according to formula (1):
Zn%=C
t* V*100/m formula (1)
C
tzinc concentration in the-sample solution that detects, mg/L;
The volume of V-sample solution, L;
The quality of m-rubber, mg.
Wherein, described in preferred steps (1), Zinc standard solution concentration range is 0 ~ 5.0mg/L.
Wherein, in preferred steps (2), sample sample weighting amount m is 120-500mg, and nitric acid addition is 8-20mL, and deionized water addition is 10-15mL, and micro-wave digestion workstation running parameter is 800W, 180 DEG C, 30min.
The mensuration wavelength of continuous light source atom absorption spectrophotometry instrument Zn is 213.857nm.
Said method of the present invention is generally used for the mensuration not containing silicon dioxide, if containing silicon dioxide in glue sample to be measured, then above-mentioned steps (2) then replaces with: (2), sample preparation and measurement
Be placed in counteracting tank by glue sample freeze grinding to be measured, gelatinous substance amount to be measured is designated as m, adds salpeter solution and hydrofluoric acid solution, and composite can is put into micro-wave digestion workstation and carried out micro-wave digestion after having assembled; After having cleared up, counteracting tank is taken out and exit in ventilation, until do not have yellow smog to emerge; Then move in volumetric flask with deionized water gradation by digestion solution, constant volume shakes up, and volume is designated as V, measures absorbance at continuum source atomic absorption spectrometer.
Compared with current national standard method (GB/T 4500-2003), method of testing provided by the invention has the following advantages:
(1) sample prepared of this method freeze grinding instrument, particle diameter is less, relatively more even again, easily clears up completely.
(2) this method does not have ashing, does not use sulfuric acid yet, reduces pollution on the environment and the injury to human body.
(3) particularly for the sample containing silicon dioxide, this method only just solves with a step micro-wave digestion interference that silicon dioxide causes, both simply, and environmental protection again.
(4) this method does not use expensive alms bowl crucible, reduces cost.
(5) the mensuration wavelength chosen of this method is more accurate, less on the Atomic absorption impact measured near wavelength.
(6) standard solution of this method is the standard solution that can directly dilute, and compares with the drafting adopting the mode of nitric acid dissolve zinc granule to carry out the typical curve of zinc in GB/T4500-2003 GB, more succinctly, fast, accurately.
Therefore, accurately the content of zinc in rubber can be made by Quick Measuring according to method of the present invention.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated.These embodiments are only for purpose of explanation, instead of limitation of the present invention.
The experimental facilities model used in the embodiment of the present invention and manufacturer see the following form shown in 1.
Table 1 experimental facilities model and manufacturer
| MM400 freeze grinding instrument | Germany's Lay is speeded Retsch GmbH |
| MARS micro-wave digestion/abstraction instrument | U.S. CE M company |
| ContrAA300 continuous light source atom absorption spectrophotometry instrument | Analytik Jena AG |
Embodiment 1
The preparation of sample A
Formula 1 (mass parts):
Component one:
Component two: sulphur (Puyang are Simon Rex Chemical Co., Ltd. not) 2.0;
Accelerator CZ (Flexsys) 2.0;
Vulcanized rubber preparation technology: in 1.6 liters of Banbury Banbury mixeies (production of FARREL company), add component 1, mix 6 minutes, obtain masterbatch, park 20 hours in room temperature; Then use XK-160 opening rubber mixing machine (production of Qingdao Xin Chengyiming rubber manufacturing machinery company limited) to blending ingredients in masterbatch 3, to carry out mixing, thus obtain rubber composition; By composition (production of Zhen Wu town, Jiangdu district Bo Hai test machines factory) sulfuration (curing temperature 160 DEG C on BH-25T vulcanizing press obtained by said method, cure time 30min) make vulcanized rubber thin slice, obtained vulcanized rubber test sample A.The gross mass of sample A is 235 parts, and Zn content is 1.20%.
According to the Zn content in method working sample A of the present invention
(1) drawing standard curve
Step 1, accurately measure 0,0.5,1.0,1.5,2.0,2.5,3.0mL concentration is after the Zinc standard solution of 1000ug/mL (China National Measuring Science Research Inst.), join in the Glass capacity bottle of 6 100mL respectively, be settled to scale with the watery hydrochloric acid of 1%, obtain concentration be 0,0.5,1.0,1.5,2.0,2.5, the zinc standard series of 3.0ug/mL.Under the optimum of zinc measures wavelength (213.857nm), the typical curve of zinc is obtained with continuum source atomic absorption spectrometer;
Table 2
With the above results drawing standard curve, curve obtains typical curve:
Y＝(0.03775+0.50029X)/(1+0.30214X) R
2＝0.9993。
(2) sample pre-treatments and test
Step 2, take the glue sample that 0.1005g shreds, be placed in counteracting tank, add 8mL salpeter solution, composite can puts into micro-wave digestion workstation after having assembled, setup parameter 800W, 180 DEG C, 30min clears up.
Step 3, cleared up after by counteracting tank take out exit in ventilation, until do not have yellow smog to emerge, moved in 100mL volumetric flask by lysate with deionized water gradation, constant volume shakes up.Prepare blank solution simultaneously.
Step 4, be 213.857nm place working sample zinc concentration C at continuous light source atom absorption spectrophotometry instrument wavelength
t.
3, calculate
Solution absorbance value calculates zinc concentration C in sample solution on typical curve per sample
t;
The content of zinc in rubber is calculated according to formula (1):
Zn%=C
t* V*100/m formula (1)
C
tzinc concentration in the-sample solution that detects, mg/L;
The volume of V-sample solution, L;
The quality of m-rubber, mg.
Comparative example 1: according to the Zn content in GB/T 4500-2003 working sample A
(1) sample pre-treatments
Step 1, take the cured rubber samples A of preparation in preparation embodiment 1 that 0.1017g shredded in porcelain crucible, carry out calcination by the method for the rubber ash content calcination of the regulation of GB/T4498-1997, namely use microwave Muffle furnace ashing at 25 DEG C, 550 DEG C of soil complete.
Step 2, add 20mL hydrochloric acid solution (concentrated hydrochloric acid and water by volume 1:1 preparation hydrochloric acid solution) in ash content, carry out dissolving (noting the splashing that carbonate decomposition causes and foaming), with the dilute hydrochloric acid solution gradation of 1%, solution and residue are moved in beaker again, heating 30min, if residue all dissolves, solution is moved in 100mL volumetric flask, be diluted to scale with the dilute hydrochloric acid solution of 1%, shake up.Prepare blank solution simultaneously.
Step 3, typical curve use the typical curve in above embodiment.
Step 4, be 213.857nm place working sample zinc concentration at continuous light source atom absorption spectrophotometry instrument wavelength be C1.
Step 5, per sample solution absorbance value calculate zinc concentration C1 in sample solution on typical curve;
The content of zinc in rubber is calculated according to formula (1):
Zn%=C1*V*100/m formula (1)
Zinc concentration in the sample solution that C1-detects, mg/L;
The volume of V-sample solution, L;
The quality of m-rubber, mg.
Table 3
Embodiment 2
The preparation of sample B
Component 1:
Component 2:
Sulphur: (Puyang are Simon Rex Chemical Co., Ltd. not) 1.5;
Accelerator CZ: (Flexsys (Flexsys)) 1.2;
Vulcanized rubber preparation technology: in 1.6 liters of Banbury Banbury mixeies (production of FARREL company), add component 1, mix 6 minutes, obtain masterbatch, park 20 hours in room temperature; Then use XK-160 opening rubber mixing machine (production of Qingdao Xin Chengyiming rubber manufacturing machinery company limited) to blending ingredients in masterbatch 3, to carry out mixing, thus obtain rubber composition; By composition (production of Zhen Wu town, Jiangdu district Bo Hai test machines factory) sulfuration (curing temperature 160 DEG C on BH-25T vulcanizing press obtained by said method, cure time 30min) make vulcanized rubber thin slice, obtained vulcanized rubber test sample B.The gross mass of sample B is 162 parts, and Zn content is 1.73%.
According to the Zn content in method working sample B of the present invention
(1) drawing standard curve
Step 1, accurately measure 0,0.5,1.0,1.5,2.0,2.5,3.0mL concentration is after the Zinc standard solution of 1000ug/mL (China National Measuring Science Research Inst.), join in the Glass capacity bottle of 6 100mL respectively, be settled to scale with the watery hydrochloric acid of 1%, obtain concentration be 0,0.5,1.0,1.5,2.0,2.5, the zinc standard series of 3.0ug/mL.Under the optimum of zinc measures wavelength (213.857nm), the typical curve of zinc is obtained with continuum source atomic absorption spectrometer;
Table 4
With the above results drawing standard curve, curve obtains typical curve: Y=(0.03775+0.50029X)/(1+0.30214X) R
2=0.9993.
(2) sample pre-treatments and test
Step 2, take the glue sample that 0.1001g shreds, be placed in counteracting tank, add 8mL salpeter solution and 1mL hydrofluoric acid solution, composite can puts into micro-wave digestion workstation after having assembled, setup parameter 800W, 180 DEG C, 30min clears up.
Step 3, cleared up after by counteracting tank take out exit in ventilation, until do not have yellow smog to emerge, moved in 100mL volumetric flask by lysate with deionized water gradation, constant volume shakes up.Prepare blank solution simultaneously.
Step 4, be 213.857nm place working sample zinc concentration C at continuous light source atom absorption spectrophotometry instrument wavelength
t.
3, calculate
Solution absorbance value calculates zinc concentration C in sample solution on typical curve per sample
t;
The content of zinc in rubber is calculated according to formula (1):
Zn%=C
t* V*100/m formula (1)
C
tzinc concentration in the-sample solution that detects, mg/L;
The volume of V-sample solution, L;
The quality of m-rubber, mg.
Comparative example 2: according to the Zn content in GB/T 4500-2003 working sample B
(1) sample pre-treatments
Step 1, take the cured rubber samples B of preparation in preparation embodiment 2 that 0.1023g shredded in platinum crucible, carry out calcination by the method for the rubber ash content calcination of the regulation of GB/T4498-1997, namely use microwave Muffle furnace ashing at 25 DEG C, 550 DEG C of soil complete.
After step 2, cooling, add several sulfuric acid, with electric hot plate or heating water bath extremely white cigarette in fuming cupboard.Add 3 sulfuric acid and 5ml hydrofluorite after slightly cold, heating, is evaporated to dry, constantly stirs with platinum rod or teflon rod, repeat twice by this step during heating.Treat that sample is cooled to room temperature, add 30mL hydrochloric acid solution (hydrochloric acid solution of concentrated hydrochloric acid and water 1:1 preparation by volume) and filter with sand core funnel, with 1% hydrochloric acid solution washing.Filtrate and cleansing solution are incorporated in 100ml, in volumetric flask, are diluted to scale with 1% hydrochloric acid solution, shake up.Prepare blank solution simultaneously.
Step 3, typical curve use the typical curve in above embodiment.
Step 4, be 213.857nm place working sample zinc concentration at continuous light source atom absorption spectrophotometry instrument wavelength be C
1.
Step 5, per sample solution absorbance value calculate zinc concentration C in sample solution on typical curve
1;
The content of zinc in rubber is calculated according to formula (1):
Zn%=C
1* V*100/m formula (1)
C
1zinc concentration in the-sample solution that detects, mg/L;
The volume of V-sample solution, L;
The quality of m-rubber, mg.
Table 5
Claims (5)
1., by a method for Zn content in atomic absorption spectrometry rubber, it is characterized in that, comprise the following steps:
(1), drawing standard curve
Prepare 6 ~ 8 different zinc standard series, test with continuum source atomic absorption spectrometer, obtain the typical curve about zinc concentration and absorbance;
(2), sample preparation and measurement
Be placed in counteracting tank by glue sample freeze grinding to be measured, gelatinous substance amount to be measured is designated as m, adds salpeter solution, and composite can is put into micro-wave digestion workstation and carried out micro-wave digestion after having assembled; After having cleared up, counteracting tank is taken out and exit in ventilation, until do not have yellow smog to emerge; Move in volumetric flask with deionized water gradation by digestion solution, constant volume shakes up, and volume is designated as V, measures absorbance at continuum source atomic absorption spectrometer;
(3), calculate
On the typical curve of step (1) gained, corresponding zinc concentration C is searched according to the sample solution absorbance of step (2) gained
t;
The content of zinc in rubber is calculated according to formula (1):
Zn%=C
t* V*100/m formula (1)
C
tzinc concentration in the-sample solution that detects, mg/L;
The volume of V-sample solution, L;
The quality of m-rubber, mg.
2. according to the method for claim 1, it is characterized in that, described in step (1), Zinc standard solution concentration range is 0 ~ 5.0mg/L.
3. according to the method for claim 1, it is characterized in that, in step (2), sample sample weighting amount m is 120-500mg, and nitric acid addition is 8-20mL, deionized water addition is 10-15mL, and micro-wave digestion workstation running parameter is 800W, 180 DEG C, 30min.
4. according to the method for claim 1, it is characterized in that, the mensuration wavelength of continuous light source atom absorption spectrophotometry instrument Zn is 213.857nm.
5. according to the method for claim 1, it is characterized in that, if containing silicon dioxide in glue sample to be measured, then above-mentioned steps (2) then replaces with as follows:
(2), sample preparation and measurement
Be placed in counteracting tank by glue sample freeze grinding to be measured, gelatinous substance amount to be measured is designated as m, adds salpeter solution and hydrofluoric acid solution, and composite can is put into micro-wave digestion workstation and carried out micro-wave digestion after having assembled; After having cleared up, counteracting tank is taken out and exit in ventilation, until do not have yellow smog to emerge; Then move in volumetric flask with deionized water gradation by digestion solution, constant volume shakes up, and volume is designated as V, measures absorbance at continuum source atomic absorption spectrometer.
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| CN110095419A (en) * | 2019-04-20 | 2019-08-06 | 上海华谊检验检测技术有限公司 | The detection method of lead, cadmium in automotive material |
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